Process for manufacturing nitrogen compounds.



E.- KOCHENDOERFER. PROCESS 50R MANUFACTURING NITROGEN COMPOUNDS.

APPLICATION FILED OCT. 31, I912.

1,165,358. Patented Deg. 21, 1915.

p; '/B 1 J3 culations.

ITED STATES PATENT orrro ERNST KOCHENDOERFER, OF FRANKFORT- ON-THE-MAIN. GERMANY.

PROCESS FOR.MANT.lFACTURING NITROGEN COMPOUNDS.

Specification of Letters Patent.

Patented Dec. 21, 1915.

Application filed October 31, 1912. Serial No. 728,762.

To all whom/it may concern:

' Be it known that 1, ERNST KocHENnonnmm. a subject of the Emperor of Germany, residing at Frankfort-on-the-Maln, Germany, have invented certain new and useful Improvements in Processes for Manufacturing Nitrogen Compounds.

known cyanization of certain gases, result- ,ing from the carbonization of distillers wash and the like, by means of over-heating; said gases have a considerable content of nitrogen, which renders them "ery valuable for the manufacture of nitrogen compounds such as cyanogen compounds and ammonia. There are quite a number of processes for such manufacture, but these processes are not sufficiently satisfactory because the yield of nitrogen compounds is considerably below that to be expected on theoretical cal-- The gases resulting from the.

carbonization of distillers. wash, hereinafter simply called gases, consist of a great number of different organic substances, of which, however, only a part carry nitrogen as a constituent of their body; the latter organic substances forming a part of the gases, and characterized by their content of nitrogen, may be called nitrogen-carriers. These nitrogen-carriers mainly con- 7 sist of alkylamins, resultin from the destructive distillation of bet-am and furthermore. of a great number of "complex compounds, mostly. of unknown constitution, obtained by the destructive distillationof albumins and other nitrogen-containing compounds found in the distillers wash. There is an important difference, however, in the behavior of these nitrogen-carriers, inasmuch as the alkylamins at the suitable temperature easily split up into valuable products Without any formation of carbon, whereas the other nitrogen-carriers have the tendency to split up to a much greater extent, forming much carbon, which deposits in the reaction vessel, and free nitrogen gas. The transformation of these mtro} gencarriers into substances available for commercial use, as for instance into hydrocyanic acid, is an endothermic process taking place at a high temperature. Just as in all endothermic reactions, the cya-nization of the respective gases resulting from the carbonization of distillers wash does not occur suddenly in an explosive manner, whereas on the other hand, the reaction is very much' better, because of its slowness, than has usually been supposed up to the present tlme.

At the present state of the art it has been considered as essential for the success of the operation to have the gases come as often and as much as possible into contact with All the present the-walls of the heater. processes for the cyanization of gases resulting from the carbonization of distillers wash acknowledge this principle as a prime condition, inasmuch as the super-heater channels, with an inside lining having a rough surface for a close contact of the gases with the walls during the c'yanizing process (German Patent 86913), were substituted by such channels provided with a filler (German-Patent 113530), allowing a close and intimate contact of the gases with the hot filler and hence a more perfect exposure to the heat.

Contrary to the accepted standpoint, .I have found that it is-of'great importance for. the economical success of the cyanizing process to convey the necessary heat for the reaction to the gases as much as possible, by

radiation from, rather than by contact with, the walls. To create .the best conditions for heating the gases, as much as possible, by radiating heat, it is necessary 'that the gases, in passing into the reaction vessel, meet as little resistance as possible; attention must be given that the gases are not exposed to friction with the rough inside surfaces of the super-heated channels,

nor should they come into contact with any obstruction such as is offered by the fillers of the old processes.-

The purpose in view is conveniently obtained by my method wherein I avoid the use of fillers in the super-heater channels and conduct the gases through empty channels which are heated from the outside; a material point, however, in which,my method differs from those of the prior art, consists in the fact that I provide the inside of the channels of suitable refractory material with smooth surfaces which, even at the prevailing temperature, retain their smoothness as well as their ,density, and are free from any tendency to become porous. The result of this precaution is a most satisfactory yield'of hydrocyanic acidv as well as of' ammonia, inso far as the total yield of vitrification and furthermore are not liable to dissolutionor chemical action by the-various constituents of the distillation gases.

The Walls of the superheater channels consisting preferably of either vitrified silica or, of a vitrified mixture of'silica and-zirconia, are naturally always smooth and non porouslikeqglass and the distillation gases are therefore protected against the per: nicious influence of contactmaterial leading to .destruction of a considerable part of the gases'as the'ihigh resistance of the.walls prevents the formation of such fcontact materialwhich in the prior art wasyalways.

present in the form of scales crumbling from the Walls min the form of efiiorescences exuding therefrom. For the further elucidation of my invention a construction of the apparatus preferred for carrying out the process is illustrated, by way of example, in the accompanying drawing.

The distiller-s wash is carbonized in the. fire clay retorts'A and the distillation gases escape through'connection pipes B into the main pipe C through which they travel into a quartz tube D surrounded by a suitable mantle E made of fire clay bricks or other suitable material. As the quartz-tube D is heated to a high temperature, flue-s F of sufiicient width are interposed between the mantle E and quartz-tube D and an inlet G and en it'H is provided for the heating gases. The distillation gases are cyanized while passing through the hot quartz-tube, and leave through exit I to be further treated to assume marketable form.

' The process as described is particularly valuable in manufacturing nitrogen com pounds, such .as cyanogen compounds'and ammonia, and under the -term nitrogen compounds as used-in the claims, I mean to include cyanogen and ammonia, as well as other compounds coming within that broad designation.

Hay ng described claim and desire to my invention, what I secure by Letters 'Patnti 1. The process of manufacturing nitrogen compounds consisting in. transforming the nitrogen-carrying gases generated by the 'nels, exposing the gases durin non-porosity.

' high tempo nitrogen carrying substances, into a nitrogen compound by. conducting said gases through unobstructed, highly heated chantheir pas-' sage through said channels to heat radiating from the walls of "said channelsand reducing the friction-of the gases with the walls of the channels by lining the inside ofthe latter, with a smooth and non-porous glasslike material maintaining. smoothness and non-porosity at the high temperature of the process. Y

2-. In the process of manufacturing'nitro-. gen compounds from: the gases generated by the carbonization of distillers wash and the like nitrogenous substances, the transformation ofthe. nitrogen-carrying gases into a nitrogen cdmpound superhe'ating the gases withinthe-walls of highly heated channels, consisting of smooth vitrified acid material resistant to the constituents of the gases; i 1 3. In the process of manufacturing nitrogen compounds from the gases generated by the carbonization of distillers wash and the 7 like nitrogenous substances, the transformation of the nitrogen-carrying gases into a nitrogen compound by superheating the gases within walls having glass-like smoothness. 1 o w y 4. In the process of manufacturing nitrogen compounds from the gases generated by the carbonization of distillers wash and the like nitrogenous substances, the transformathe carbonization of distillers wash and the tion of the nitrogen-carrying gases into a nitrogen compound by superheating the gases within walls made ofmaterial retaininga glass-like smoothness at the high temperature necessary for carrying out the process.

6. In the process of manufacturing nitrogen compounds from the gases generated by the carbonization of distillers wash andthe like nitro enous substances,.the transformation oft-lie nitrogen-carrying gases into a nitrogen compound by supe'rheating. the gases within smooth walls madeof material retaining a glass-like non-porosity at the I rature necessary for carrying 'out the process. I

7. In the process of manufacturing nitrogen compounds from the gases generated by,

- the carbonization ofidistillers wash and thegases within walls of superheatenchannels smooth inside and made of material tree from any tendency to. become porous at the high temperaturenecessary for carrying out the process.

S. In the process of manufacturing nitrogen compounds from the gases generated by the carbonization of distillers wash and the like nitrogenous substances, the transformation of the nitrogen-carrying gases into a nitrogen compound by superheating the gases within smooth non-porous walls of superheater channels consisting of vitrified oxids.

9. In the process of manufacturing nitrogen compounds from the gases generated by the carbonization of distillers wash and the like nitrogenous substances, the transformation of the nitrogencarrying gases into a nitrogen compound by superheatmg the gases within smooth non-porous walls of superheater channels consisting of vitrified oxids comprising zirconia.

10. In the process of manufacturing nitrogen compounds from the gases generated by the carbouization of distillers wash and the like nitrogenous substances, the transformation of the nitrogen-carrying gases into a nitrogen compound by superheating the gases within smooth non-porous Walls of superheater channels consisting of vitrified oxids cmuprising silicon dioxid.

In testimony whereof I have signed this specification in the presence of two subscrib ing witnesses.

n ERNST KOGHENDOERFER. Witnesses CARL BIcKsTAHL, ERNST BERMAN.

Copies of this patent may be obtained for five cents each, by addressing the Commissioner of Patents, Washington, I), C. 

